Method of preparing tungsten and alloys thereof.



NO DIaWIng.

f UNITED s rEs PATENT OFFICE.

- FREDERICK 'M. BEOKET, or mnean aranns, NEW YORK, nssrerron ro'ntno'rno METALLURGICAL oomramr, or NIAGARA rams, ns'w ronx, A oonroaa'non or WEST VIRGINIA. J

' METHOD OF PREPARING TUNGSTEN AND ALLOYS THEREOF.

To all whom it may concern Be it known that I, FREDERICK M. BEGKET,

' low-phosphorus content. The term ores is herem employed to include concentrates;

invention being the provision of methods wherebysuch ores may be utilized for the preparation of tungsten metal or alloys of I have found that certain ores oftungsten, including ferberite from Boulder county, Colorado, contain very considerable proportions of phosphorus, which. in special cases x-may attaln 0.6 to 0.7 per cent. Such ores .consist largely of iron tungstate with a gangue of 'silicious character, the phoshorus being usually associated both with the mineral and. the gangue in extremely I variable proportions. Ores presenting similar conditions are wolframite, an iron tungstate containing considerable manganese, and hiibnerlte, an iron-manganese tungstate in WhlCll manganese largely predomlnates.-

- Such ores are herein referred to as ores of the iron-tungstate typed According to the present method, the tungsten ore, or concentrate, 1s first subjected to a reducing operation, appropriate v v reducing-agents belng for example carbon,

hydrogen, carbon monoxid, producer-gas, or

furnace gases having a reducing character. The reduction is effected under known conditions at a temperature below the meltingpoint of the reduced product, and the reduction maybe either partial, approximately complete, or complete, according to circumstances. The product of this reducing oper-- ation, hereinafter referred to as the reduced product, is next subjected to treat-' ment for the removal of phosphorus. Pref erably, this is accomplished by treatment with an acid or acid-reacting body, forexample, by treating the ore with concentrated Specification 0! Letters Patent.

' Application filed May 26, 1913. Serial No. 770,031.

Patented Dec. 16', 1913.

of 200 centimeters of acid per kilogram of ore, as described in my copending application Serial No. 727,215, filed October 22,

1913, or as follows :To the reduced product 1 is added an excess of dilute sulfuric acid, say one to five per cent. concentration, and the mass is allowed to stand for some hours or is agitated with the acid solution. Mod

erate'hcating accelerates the action of the acid in removing phosphorus, but involves slight losses of tungsten by solution. The conditions are in all cases so controlled as to I increase the ratio of tungsten to phosphorus.

The acid is then drained ofl and applied'to thepurification of successive batches of reduced product, with such reinforcement as may be required. By this treatment a large proportion of the phosphorus is removed,

Instead of the above-describedacid-treat ment, any other appropriate procedure for removing phosphorus may be used. In case the initial reduction of the mass was complete or substantially complete, the purified product is now melted in an electric furnace,

vielding directly a commercially available low-phosphorus metal or ferroalloy, the composition of which depends upon the amount of residual iron. In case the initial reduction was partial or incomplete, the Ieduced product is subjected to a further or supplementary reducing operation, 1prefer-- a ly in the electric furnace, in accordance with methods now well known to those skilled in the art, and preferably by means ofa non-carbonaceous reducing agent, such as silicon, whereby there is also obtained a. low-phosphorus metal or ferroalloy, which is likewise low in carbon. I claim I 1. The method of preparing low-phosphorus tungsten or ferrotungsten, which consists in subjecting phosphorous-bearing ores of the iron-tungstate type to a reducing operation, and treating the reduced product 100 to increase the ratio of tungsten to phosphorus. Y

-sulfuric acidrin the approximate proportions 2. The method of preparing low-phos- In testimony whereoffI afiix my signature phorus tungsten or ferrotungsten, which in presence of two Witnesses.

consists in partially reducing ores of the iron-tungstate type, treating the reduced FREDERICK BECKET' 5 product to increase the ratio of tungsten to Witnesses:

phosphorus, and thereafter completing the T. L. SEOORD,

reduction. D. BURGESS. 

